WO2017033374A1 - Composition de revêtement électroconductrice, matériau électroconducteur, et leurs procédés de production - Google Patents

Composition de revêtement électroconductrice, matériau électroconducteur, et leurs procédés de production Download PDF

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WO2017033374A1
WO2017033374A1 PCT/JP2016/003049 JP2016003049W WO2017033374A1 WO 2017033374 A1 WO2017033374 A1 WO 2017033374A1 JP 2016003049 W JP2016003049 W JP 2016003049W WO 2017033374 A1 WO2017033374 A1 WO 2017033374A1
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intercalation compound
metal particles
coating composition
graphite intercalation
graphite
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Japanese (ja)
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忠政　明彦
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パナソニックＩｐマネジメント株式会社
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Priority to JP2017536181A priority Critical patent/JPWO2017033374A1/ja
Priority to US15/739,686 priority patent/US20180171161A1/en
Priority to CN201680037596.XA priority patent/CN107849395A/zh
Publication of WO2017033374A1 publication Critical patent/WO2017033374A1/fr

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    • C09D179/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09D161/00 - C09D177/00
    • C09D179/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
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    • C09D7/40—Additives
    • C09D7/66—Additives characterised by particle size
    • C09D7/69—Particle size larger than 1000 nm
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20—Conductive material dispersed in non-conductive organic material
    • H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20—Conductive material dispersed in non-conductive organic material
    • H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
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Definitions

  • the present invention relates to a conductive composite material, and more particularly to a conductive coating composition using a graphite intercalation compound, a conductive material, a method for manufacturing a conductive coating composition, and a method for manufacturing a conductive material.
  • One material that achieves high conductivity is a metal material such as silver.
  • the unit price of a metal material is generally high. Therefore, it is required to further improve conductivity while using a graphite intercalation compound whose unit price is relatively low.
  • the present invention has been made in view of such a situation, and an object thereof is to provide a technique for improving conductivity while suppressing an increase in unit price.
  • a conductive coating composition is a conductive coating composition including a graphite intercalation compound, metal particles, a binder, and a solvent, wherein the conductive coating composition The volume occupied by the graphite intercalation compound in the product is larger than the volume occupied by the metal particles in the conductive coating composition.
  • This conductive material is a conductive material containing a graphite intercalation compound and metal particles, and the volume occupied by the graphite intercalation compound in the conductive material is larger than the volume occupied by the metal particles in the conductive material.
  • Still another embodiment of the present invention is a method for producing a conductive coating composition.
  • a graphite intercalation compound and metal particles are mixed to produce a conductive material, a binder and a solvent are stirred and heated to produce a binder solution, and the binder solution is electrically conductive.
  • a volume of the graphite intercalation compound in the conductive coating composition is larger than a volume of the metal particles in the conductive coating composition.
  • Still another aspect of the present invention is a method for producing a conductive material.
  • This method is a method for producing a conductive material in which a graphite intercalation compound and metal particles are mixed, and the volume occupied by the graphite intercalation compound in the conductive material is larger than the volume occupied by the metal particles in the conductive material.
  • the conductivity can be improved while suppressing an increase in unit price.
  • Embodiments of the present invention relate to a conductive material containing a graphite intercalation compound and a conductive coating composition using the conductive material.
  • the metal material has high conductivity, but its material unit price is high.
  • the unit price of the carbon material is low, but its conductivity is low.
  • the graphite intercalation compound has a relatively high conductivity while being inexpensive. Therefore, it is required to improve the conductivity of the graphite intercalation compound.
  • metal particles are bonded to the graphite intercalation compound.
  • FIG. 1 shows a configuration of a conductive coating composition 100 according to an embodiment of the present invention.
  • the conductive coating composition 100 includes a graphite intercalation compound 10 and metal particles 20.
  • the conductive coating composition 100 includes a binder and a solvent (not shown) in order to bond them. It can be said that the graphite intercalation compound 10 and the metal particles 20 are conductive materials.
  • the graphite intercalation compound 10 is a compound having a sandwich structure in which various atoms, molecules, and the like are intruded into the interlayer of graphite, which is a layered material in which carbon hexagonal network surfaces are laminated in parallel.
  • the number of conductive carriers on the graphite layer increases due to charge transfer between the intercalation such as atoms and molecules that have entered between the graphite layers and the adjacent graphite layer. As a result, the graphite intercalation compound 10 has high conductivity.
  • the graphite intercalation compound 10 uses, for example, powders such as flaky natural graphite, artificial graphite, vapor-grown carbon fiber, and graphite fiber as a base material.
  • the graphite intercalation compound 10 may be based on, for example, a pyrolytic graphite sheet obtained by heat-treating a polyimide film at 2600 to 3000 ° C. or a material obtained by pulverizing a pyrolytic graphite sheet.
  • the graphite intercalation compound 10 may be based on a graphite material having good crystal integrity such as a metal supported on the end of these graphite materials. In order to support the metal on the end of the graphite material, for example, the metal complex and the graphite material are mixed and then fired. Note that the base material is not limited to these.
  • any substance species such as atoms, molecules, and ions can be used as intercalation, and for example, metal chloride, alkali metal, and alkaline earth metal are used.
  • metal chlorides are iron chloride, copper chloride, nickel chloride, aluminum chloride, zinc chloride, cobalt chloride, gold chloride, bismuth chloride, etc.
  • alkali metals and alkaline earth metals are lithium, potassium, rubidium Cesium, calcium, magnesium and the like. In addition, two or more of these may be used in combination as intercalation.
  • the graphite intercalation compound 10 in which the metal chloride is inserted is heat-treated at 250 to 500 ° C.
  • intercalate inserted into graphite is iron chloride or copper chloride having a high electron affinity, it functions as an acceptor that gives holes to the graphite intercalation compound 10.
  • the intercalate inserted into the graphite functions as a donor that gives electrons to the graphite intercalation compound 10 when the ionization potential is lithium, potassium, or cesium smaller than that of graphite.
  • Metal powder is used for the metal particles 20.
  • the metal powder include stainless steel, titanium oxide, ruthenium oxide, indium oxide, aluminum, iron, copper, gold, silver, platinum, titanium, nickel, magnesium, palladium, chromium, tin, tantalum, and niobium.
  • the metal particles 20 may be a metal silicide-based conductive ceramic, a metal carbide-based conductive ceramic, a metal boride-based conductive ceramic, or a metal nitride-based conductive ceramic.
  • metal silicide-based conductive ceramics are iron silicide, molybdenum silicide, zirconium silicide, titanium silicide, and the like.
  • metal carbide based conductive ceramics include tungsten carbide, silicon carbide, calcium carbide, zirconium carbide, tantalum carbide, titanium carbide, niobium carbide, molybdenum carbide, vanadium carbide, and the like.
  • metal boride-based conductive ceramics include tungsten boride, titanium boride, tantalum boride, zirconium boride and the like.
  • metal nitride-based conductive ceramics examples include chromium nitride, aluminum nitride, molybdenum nitride, zirconium nitride, tantalum nitride, titanium nitride, gallium nitride, niobium nitride, vanadium nitride, boron nitride, and the like.
  • the metal particles 20 may be a synthetic powder using two or more of these metal powders in combination.
  • the form of the metal particle 20 is a fiber or powder obtained by depositing or plating a metal on an inorganic / organic fiber.
  • Polyester resin vinyl resin, phenol resin, acrylic resin, epoxy resin, polyimide resin, cellulose, etc. are used for the binder. Moreover, it is not limited to these.
  • Solvent is also called solvent.
  • the solvent it is preferable to contain 50% by mass or more of a solvent having a boiling point of 150 ° C. or higher, particularly a solvent having a boiling point of 200 ° C. or higher.
  • a solvent having high affinity with an inorganic substance (metal or the like) and dissolving an additive described later is preferable, and generally an organic solvent having an alcoholic OH group is preferable.
  • organic solvent is alcohol.
  • examples of alcohols include non-aliphatic alcohols such as ⁇ -terpineol; butyl carbitol (diethylene glycol monobutyl ether), hexylene glycol (2-methyl-2,4-pentanediol), ethylene glycol-2-ethylhexyl ether, etc. Glycols and the like.
  • N-methylpyrrolidone, dimethylformamide, dimethyl sulfoxide, cyclohexane and the like are preferably selected in accordance with the affinity for carbon and metal particles 20.
  • solvents with low viscosity such as aliphatic alcohols and ketones may be used, and ethanol, 2-propanol, methyl ethyl ketone, methyl isobutyl ketone, etc. are used. Also good.
  • a mixture of a high boiling point solvent and a low boiling point solvent may be used as the solvent. At that time, the ratio of the contents is not particularly limited, but as described above, the amount of the high boiling point solvent is preferably 50% by mass or more.
  • metal carbide exists as an additive between the graphite intercalation compound 10 and the metal particles 20. Therefore, the graphite intercalation compound 10 is covalently bonded or ionically bonded to the metal carbide, and the metal particles 20 are covalently bonded or ionically bonded to the metal carbide.
  • the volume occupied by the graphite intercalation compound 10 in the conductive coating composition 100 is larger than the volume occupied by the metal particles 20 in the conductive coating composition 100.
  • the volume occupied by the graphite intercalation compound 10 in the conductive coating composition 100 is 35%, and the volume occupied by the metal particles 20 in the conductive coating composition 100 is 15%.
  • the ratio is not limited to this.
  • any metal can be used as the metal particle 20, for example, use of gold, silver, or copper is preferable.
  • Their coefficients of thermal expansion [10 ⁇ 6 / K] are “14.3” (gold), “18.0” (silver), and “16.8” (copper).
  • the expansion coefficient [10 ⁇ 6 / K] is “4.4”.
  • the density [g / cm 3 ] of the metal particles 20 is “19.3” (gold), “10.5” (silver), “9.0” (copper), and the density of the graphite intercalation compound 10 [G / cm 3 ] is “2.2 to 2.4”.
  • the volume occupied by the metal particles 20 is larger than the volume occupied by the graphite intercalation compound 10
  • the coefficient of thermal expansion increases, so that peeling from peripheral members such as a substrate is likely to occur.
  • the soft material increases, the material is easily deformed, resulting in insufficient adhesion or peeling due to external force or temperature change.
  • the density increases, so the weight increases.
  • the cost increases.
  • the volume occupied by the graphite intercalation compound 10 is made larger than the volume occupied by the metal particles 20.
  • the volume occupied by the graphite intercalation compound 10 is larger than the volume occupied by the metal particles 20 in the conductive material.
  • the volume occupied by the graphite intercalation compound 10 in the conductive material is 70%
  • the volume occupied by the metal particles 20 in the conductive material is 30%. The ratio is not limited to this.
  • the average particle diameter of the metal particles 20 is made smaller than 100 ⁇ m.
  • the average particle diameter is measured by an optical microscope or a scanning electron microscope.
  • the average particle diameter that is, the size and the diameter of the metal particles 20 is reduced, the substantial melting point of the metal particles 20 is lowered.
  • the conductivity of the conductive coating composition 100 is improved.
  • the average particle size of the metal particles 20 is 100 ⁇ m or more, the phenomenon of necking becomes difficult to occur.
  • a graphite intercalation compound 10 is produced.
  • a graphite material as a raw material for the graphite intercalation compound 10 is prepared.
  • This graphite material has a layered structure formed by a graphene laminate.
  • chemical species to be intercalated are inserted between the layers of the graphite material.
  • the chemical species to be inserted is composed of the aforementioned materials.
  • a known technique such as a gas phase method or a liquid phase method is used.
  • vapor phase method vapor of a chemical species is brought into contact with graphite as a host at a high temperature.
  • the host graphite is immersed in a solution in which a chemical species is dissolved in an organic solvent or a liquid in which a chemical species is melted at a high temperature.
  • the conductive material which is a mixture is produced
  • it mixes uniformly using a ball mill, a triple roll, an extruder, a Banbury mixer, a V blender, a kneader, a ribbon mixer, a Henschel mixer, etc. Note that the generation of the conductive material is not limited to this.
  • a binder and a solvent are added to a container having a stirrer and a heating device, and a binder solution is produced while stirring and heating.
  • the conductive material is dispersed in the binder solution by adding and mixing and kneading the conductive material to the binder solution, and the conductive coating composition 100 is manufactured. Furthermore, you may manufacture a conductive wiring by baking the conductive coating composition 100.
  • Example 1 First, 2 g of iron chloride (99.9%) is dissolved in 125 mL of ethanol (special grade 99.5%), and 9.61 mL of pentaethylenehexamine (ethyleneamine mixture) is added to the Fe-N complex. Formed. To this solution, 4.0 g of natural graphite made of Ito graphite having an average particle diameter of 10 ⁇ m was added as graphite, and then dispersed by an ultrasonic homogenizer. After dispersion, ethanol was immediately removed by a rotary evaporator, and the solid content was taken out.
  • ethanol special grade 99.5%
  • pentaethylenehexamine ethyleneamine mixture
  • a quartz tube ( ⁇ 16 mm, L500 mm) in the shape of a stoppered test tube is filled with solid content, and a mixed gas of 1% O 2 /99% N 2 is mixed at 300 mL / min for 90 seconds at 900 ° C.
  • the graphite carrying iron was recovered. Iron is supported by graphite by nitrogen atoms. Impurities remaining on the surface were removed by washing the iron-supported graphite with ultrapure water.
  • 0.06 g of graphite carrying iron, 0.26 g of potassium chloride, and 0.6 g of anhydrous copper (II) chloride were vacuum sealed in a glass ampule, and the ampule was heat-treated at 400 ° C. for 10 hours. After natural cooling, graphite was taken out from the ampule, and potassium chloride and copper (II) chloride adhering to the surface were removed by washing with water to obtain a graphite intercalation compound 10.
  • a Sigma-Aldrich silver powder having an average particle diameter of 2 ⁇ m is prepared.
  • a conductive material as a material was obtained.
  • 0.1 g of the conductive material was put in a cylindrical mold having a diameter of 10 mm, and a pressure of 200 MPa was applied to obtain a green compact of the cylindrical conductive material.
  • Example 2 Instead of graphite carrying iron in Example 1, natural graphite made of Ito graphite having an average particle diameter of 10 ⁇ m was used. The rest is the same as in the first embodiment.
  • the volume resistivity of the green compact of the conductive material in each of Example 1, Example 2, and Comparative Example is measured by a four-probe method.
  • the volume resistivity in Example 1 is 18 [ ⁇ cm]
  • the volume resistivity in Example 2 is 45 [ ⁇ cm]
  • the volume resistivity in the comparative example is 120 [ ⁇ cm]. From this, the volume resistivity of Example 1 and Example 2 becomes low compared with a comparative example.
  • the graphite intercalation compounds 10 can be connected by the metal particles 20. Moreover, since the graphite intercalation compounds 10 are connected to each other by the metal particles 20, the conductivity can be improved. Moreover, since the graphite intercalation compound 10 is used, the raise of a unit price can be suppressed. Moreover, since the metal chloride is intercalated in the graphite intercalation compound 10, electroconductivity can be improved. Moreover, since the average particle diameter of the metal particles 20 is smaller than 100 ⁇ m, it is possible to easily form a conductive path. Further, since the conductive path can be easily formed, the conductivity can be improved.
  • the conductivity can be improved.
  • the volume occupied by the graphite intercalation compound 10 in the conductive material is larger than the volume occupied by the metal particles 20, the graphite intercalation compounds 10 can be connected by the metal particles 20.
  • the low-cost and highly conductive graphite intercalation compound 10 is used, so that the cost can be reduced while maintaining high conductivity characteristics.
  • the graphite intercalation compound 10 is bonded using a small amount of metal particles 20, high conductivity that cannot be obtained by conventional carbon-based wiring can be obtained.
  • nitrogen atoms exist between the graphite intercalation compound 10 and the metal particles 20, iron is easily supported by graphite, and the metal particles 20 can be easily bonded to the graphite intercalation compound 10.
  • a conductive coating composition 100 is a conductive coating composition 100 including a graphite intercalation compound 10, metal particles 20, a binder, and a solvent.
  • the volume occupied by the intercalation compound 10 is larger than the volume occupied by the metal particles 20 in the conductive coating composition 100.
  • the graphite intercalation compound 10 may be intercalated with a metal chloride.
  • the average particle diameter of the metal particles 20 is smaller than 100 ⁇ m.
  • the graphite intercalation compound 10 and the metal particles 20 may be chemically bonded.
  • Nitrogen atoms may exist between the graphite intercalation compound 10 and the metal particles 20.
  • Metal carbide may exist between the graphite intercalation compound 10 and the metal particles 20.
  • the graphite intercalation compound 10 may be covalently bonded or ionically bonded to the metal carbide, and the metal particle 20 may be covalently bonded or ionically bonded to the metal carbide.
  • This conductive material is a conductive material including the graphite intercalation compound 10 and the metal particles 20, and the volume occupied by the graphite intercalation compound 10 in the conductive material is larger than the volume occupied by the metal particles 20 in the conductive material. .
  • Still another embodiment of the present invention is a method for producing the conductive coating composition 100.
  • the graphite intercalation compound 10 and the metal particles 20 are mixed to produce a conductive material, the binder and the solvent are stirred and heated to produce a binder solution, and the binder solution.
  • Still another aspect of the present invention is a method for producing a conductive material.
  • This method is a method for producing a conductive material in which graphite intercalation compound 10 and metal particles 20 are mixed, and the volume occupied by graphite intercalation compound 10 in the conductive material is larger than the volume occupied by metal particles 20 in the conductive material. Is also big.
  • the conductivity can be improved while suppressing an increase in unit price.

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Abstract

Cette invention concerne une composition de revêtement électroconductrice 100 contenant un composé d'intercalation du graphite 10, des particules métalliques 20, un liant et un solvant. Le composé d'intercalation du graphite 10 a une structure en sandwich obtenue en faisant pénétrer divers atomes, molécules, et autres entre les feuillets du graphite, qui est un matériau en feuillets dans lequel les plans du réseau hexagonal du carbone sont empilés en parallèle. Le liant et le solvant lient le composé d'intercalation du graphite 10 et les particules métalliques 20 ensemble. Le volume occupé par le composé d'intercalation du graphite 10 dans la composition de revêtement électroconductrice 100 est supérieur au volume occupé par les particules métalliques 20 dans la composition de revêtement électroconductrice 100.
PCT/JP2016/003049 2015-08-24 2016-06-24 Composition de revêtement électroconductrice, matériau électroconducteur, et leurs procédés de production WO2017033374A1 (fr)

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JP2017536181A JPWO2017033374A1 (ja) 2015-08-24 2016-06-24 導電性塗料組成物、導電性材料、導電性塗料組成物の製造方法、導電性材料の製造方法
US15/739,686 US20180171161A1 (en) 2015-08-24 2016-06-24 Conductive coating composition, conductive material, method for manufacturing conductive coating composition, and method for manufacturing conductive material
CN201680037596.XA CN107849395A (zh) 2015-08-24 2016-06-24 导电性涂料组合物、导电性材料、导电性涂料组合物的制造方法、导电性材料的制造方法

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CN108744985A (zh) * 2018-05-16 2018-11-06 南京帝膜净水材料开发有限公司 一种卷式膜元件
CN108706575B (zh) * 2018-07-06 2019-12-31 广州特种承压设备检测研究院 一种液相球磨剥离石墨烯的制备方法
CN111114041A (zh) * 2020-01-07 2020-05-08 中国电子科技集团公司第十六研究所 一种高导热石墨-铜互穿式结构的复合材料及制备方法
CN116313219A (zh) * 2023-02-23 2023-06-23 华中科技大学 一种导电浆料及其制备方法与在多孔背电极中的应用

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JPH0565366A (ja) * 1991-09-06 1993-03-19 Yazaki Corp 導電性樹脂組成物

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JPH0195170A (ja) * 1987-10-06 1989-04-13 Yamaha Corp 導電性塗料
JPH09249407A (ja) * 1996-03-14 1997-09-22 Toyota Central Res & Dev Lab Inc 黒鉛複合物およびその製造方法
JP5151150B2 (ja) * 2006-12-28 2013-02-27 株式会社日立製作所 導電性焼結層形成用組成物、これを用いた導電性被膜形成法および接合法
JP5039514B2 (ja) * 2007-11-16 2012-10-03 ハリマ化成株式会社 低抵抗導電性ペースト
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JPH0565366A (ja) * 1991-09-06 1993-03-19 Yazaki Corp 導電性樹脂組成物

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